高效液相色谱法测定通经甘露丸中大黄酸、大黄素及大黄酚含量

目的建立测定通经甘露丸中大黄素、大黄酚及大黄酸含量的高效液相色谱法。方法采用DiamonsilC18色谱柱（250mm×4.6mm,5μm）,流动相为甲醇-0.1%磷酸溶液（85：15）,流速1.0mL/min,检测波长254nm。结果大黄酸进样量在0.0924～0.2464μg范围内与峰面积线性关系良好,r=0.9998,平均加样回收率为98.45%,RSD为0.82%（n=6）;大黄素进样量在0.0576～0.1536μg范围内与峰面积线性关系良好,r=0.9999,平均加样回收率为98.76%,RSD为1.15%（n=6）;大黄酚进样量在0.1397～0.3725μg范围内与峰面积线性关系良好,r=0.9998,平均加样回收率为99.03%,RSD为0.91%（n=6）。结论高效液相色谱法操作简便,结果准确,重现性好,适用于通经甘露丸中大黄酸、大黄素及大黄酚的含量测定。     

HPLC法测定四黄泻火片中大黄素及大黄酚的含量

目的：建立四黄泻火片中大黄素及大黄酚的HPLC测定方法。方法：色谱柱为phenomenex C18柱（250mm×4．6mm,5μm）,流动相为甲醇-0．1％磷酸（87：13）,流速为1．0ml·min^-1,检测波长为254am．结果：大黄素在0．0332～0．1880μg范围内与峰面积呈良好线性关系（r=0．9997）,平均加样回收率为100．0％,RSD为1．1％（n=5）;大黄酚在0．0751～0．4257μg范围内与峰面积呈良好线性关系（r=0．9998）,平均加样回收率为99．9％,RSD为1．1％（n=5）。结论：方法简便、准确,专属性强,重复性好,可用于四黄泻火片的质量控制。     

HPLC法同时测定金酸萍颗粒中大黄素、大黄酚的含量

目的：建立用高效液相色谱法测定金酸萍颗粒中大黄素、大黄酚含量的方法。方法：色谱柱：Rainbow C18（250mm×4．6mm,5μm）,流动相：甲醇-0．1％磷酸溶液（85：15）,检测波长：254nm,流速：1．0ml·min^-1。结果：大黄素进样量在0．03～0．63μg范围内线性关系良好（r=0．9999）,平均回收率为99．98％（n=6）,RSD为0．40％;大黄酚进样量在0．03～0．64μg范围内线性关系良好（r=0．9999）,平均回收率为99．57％,RSD为0．45％。结论：该方法操作简单易行,专属性强,准确可靠,可用于金酸萍颗粒的质量控制。     

皮肤病血毒散质量标准研究

目的提高皮肤痛血毒散的质量标准。方法用柱层析分离技术纯化组分，对各组分与对照品同时进行薄层色谱（TLC）鉴别，用高效液相色谱（HPLC）法测定含量。结果TLC鉴别可检出9种药材。HPLC含量测定表明，大黄素进样量在0．0156—0．5μg范围内与峰面积线性关系良好，r=0．9999，大黄酚进样量在0．0313～1．0μg范围内与峰面积线性关系良好，r=0．9999。平均回收率大黄素为99．17％（RSD=1．21％），大黄酚为99．01％（RSD=1．41％）。结论所用方法简便、专属、准确、重现性好，可用于皮肤病血毒散的质量控制。     

高效液相色谱法同时测定双黄连粉针中黄芩苷和连翘苷含量

目的建立同时测定双黄连冻干粉中黄芩苷和连翘苷含量的高效液相色谱法。方法采用Hypersil-C18柱（250mm×4，6mm,5μm），流动相为甲醇-乙腈-水-磷酸（65：15：75：0，5），流速为1.0mL／min，检测波长为230nm。结果黄芩苷进样量在0，14-2，80μg范围内与峰面积线性关系良好（r=0．9998），平均回收率为98，09％，RSD=0，76％（n=6）；连翘苷进样量在0，077-1．93μg范围内与峰面积线性关系良好（r=0，9997），平均回收率为98，38％，RSD=1，11％（n=6）。结论方法专属性强、准确、快速，适用于双黄连冻干粉的质量控制。     

HPLC同时测定栀子金花丸中黄芩苷、大黄素、大黄酚的含量

目的:建立高效液相色谱法测定测定栀子金花丸中黄芩苷、大黄素、大黄酚的含量。方法:色谱柱为Diamonsil C18(250 mm×4.6 mm,5μm);流动相为甲醇-0.4%磷酸溶液,采用梯度洗脱;检测波长为254 nm:柱温:室温,流速:1.0 ml.min-1。结果:黄芩苷进样量在0.154～1.540μg范围内与峰面积线性关系良好,r=0.999 6,平均回收率为100.2%,RSD=1.5%(n=9);大黄素进样量在0.071～0.714μg范围内与峰面积线性关系良好,r=1.000 0,平均回收率为99.7%,RSD=1.2%(n=9);大黄酚进样量在0.147～1.472μg范围内与峰面积线性关系良好,r=0.999 8,平均回收率为100.0%,RSD=1.2%(n=9)。结论:该方法简便、准确、重复性好。     

高效液相色谱法测定上清丸中大黄素和大黄酚的含量

目的建立上清九中大黄素和大黄酚的含量测定方法。方法色谱柱为Diamonsil C18（250mm×4．6mm,5μm）,流动相为甲醇-0．1％磷酸溶液（85：15）,流速：1．OmL·min^-1,检测波长：254nrn。结果大黄素进样量在0．0576～0．1536μg线性关系良好,r=0．9999,平均加样回收率为98．49％,RSD为1．75％（n=6）;大黄酚进样量在0．1397～0．3725μg线性关系良好,r=0．9998,平均加样回收率为98．86％,RSD为1．24％（n=6）。结论该方法操作简便,结果准确,重现性好,适用于上清丸中大黄素和大黄酚的含量测定。     

反相高效液相色谱法测定妇康止痛片中大黄素含量

目的建立测定妇康止痛片中大黄素含量的反相高效液相色谱法。方法色谱柱为C18柱，流动相为甲醇-0，1％磷酸溶液（80：20），检测波长为288nm，流速为1，0mL／min，柱温为25℃。结果大黄素进样量在0，05～0．40μg范围内与峰面积呈良好的线性关系，r=0，9995，平均加样回收率为98，54％，RSD=1．65％（n=6）。结论所用方法结果准确可靠，操作简便，可用于妇康止痛片的质量控制。     

RP-HPLC法测定清肺抑火片的含量

建立清肺抑火片含量测定的RP-HPLC法。选用Agilent Eclipse XDB C18色谱柱，甲醇-乙腈-1．5％醋酸溶液为流动相作梯度洗脱；检测波长280nm。黄芩苷在0．12～3．60μg的范围内呈良好的线性关系，r=0．9999，平均回收率为97．58％（n=5），RSD=1．71％；大黄素在0．012～0．360μg的范围内呈良好的线性关系，r=0．9999，平均回收率为97．86％（n=5），RSD=1．81％；大黄酚在0．02～0．60μg的范围内呈良好的线性关系，r=0．9999，平均回收率为98．65％（n=5），RSD=1．88％。本法操作简便准确，测定清肺抑火片的含量，便于全面控制该制剂的质量。     

HPLC法测定肠安康颗粒中白术内酯I与苍术酮的含量

目的：建立肠安康颗粒中白术内酯I与苍术酮的含量测定方法。方法：采用高效液相色谱法,色谱柱为伊利特ODS色谱柱（250mm×4．6mm,5μm）,流动相为乙腈-水（梯度洗脱）,流速为1mL·min^-1,检测波长为220nm。结果：白术内酯I进样量在0．1～2．01μg范围内与峰面积积分值呈良好线性关系（r=0．9999）,平均回收率为98．84％,RSD=0．76％（n=6）;苍术酮进样量在0．5-10．0μg范围内与峰面积积分值呈良好线性关系（r=0．9999）,平均回收率为98．43％,RSD=1．14％（n=6）。结论：本方法简便、准确,可用于肠安康颗粒的质量控制。     

Efficacy of gut lavage,hemodialysis, and hemoperfusion in the therapy of paraquat or diquat intoxication

Clinical and in vitro investigations were carried out to test the efficacy of gut lavage, hemodialysis, and hemoperfusion in the treatment of poisoning with paraquat or diquat. In a patient suffering from diquat intoxication 130 times more diquat was removed by gut lavage 30 h after ingestion than was removed by complete aspiration of the gastric contents.Determination of in vitro clearances for paraquat and diquat by hemodialysis showed that, at serum concentrations of 1–2 ppm, such as are frequently encountered in poisoning in man, toxicologically relevant quantities of herbicide cannot be removed from the body. At a concentration of 20 ppm, on the other hand, hemodialysis proved to be effective, the clearance being 70 ml/min at a blood flow rate of 100 ml/min. The efficacy of hemoperfusion with coated activated charcoal was on the whole better. Especially at concentrations around 1–2 ppm, the clearance values for hemoperfusion were some 5–7 times higher than those for hemodialysis.In a patient suffering from paraquat poisoning, both hemodialysis as well as hemoperfusion were carried out. The in vitro results could be confirmed: At serum concentrations of paraquat less than 1 ppm no clearance could be obtained by hemodialysis while by hemoperfusion with activated charcoal quite high clearance values were measured and the serum level dropped down to zero.

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Zusammenfassung Klinische Untersuchungen und Laboratoriumsversuche wurden durchgeführt, um die Wirksamkeit von Darmspülung, Hämodialyse und Hämoperfusion bei Paraquat- und Deiquat-Vergiftungen zu prüfen.Bei einem Patienten wurde 30 Std nach Deiquat-Aufnahme durch Darmspülung 130mal mehr Deiquat entfernt als durch vollständige Aspiration des Mageninhaltes. In vitro-Versuche ergaben, daß bei Blutserumkonzentrationen von 1–2 ppm, die bei Vergiftungen oft gemessen werden, durch Hämodialyse keine toxikologisch relevanten Paraquat- oder Deiquat-Mengen entfernt werden können. Dagegen erwies sich die Hämodialyse bei 20 ppm und einer Blutumlaufgeschwindigkeit von 100 ml/min mit einer Clearance von 70 ml/min als wirksam. Die Hämoperfusion mit beschicheter Aktivkohle war in diesen Versuchen aber eindeutig überlegen, denn insbesondere bei Konzentrationen um 1–2 ppm waren die Clearance-Werte 5–7mal höher als bei der Hämodialyse.Die in vitro-Ergebnisse wurden bei einem Patienten mit einer Paraquat-Vergiftung bestätigt: Bei Konzentrationen unter 1 ppm war die Hämodialyse wirkungslos, während durch Hämoperfusion relativ hohe Clearance-Werte erreicht wurden, so daß der Serumspiegel rasch unter die Nachweisgrenze abfiel.

     

In vitro studies on sterically stabilized liposomes (SL) as enzyme carriers in organophosphorus (OP) antagonism

This study describes a new approach for organophosphorous (OP) antidotal treatment by encapsulating an OP hydrolyzing enzyme, OPA anhydrolase (OPAA), within sterically stabilized liposomes. The recombinant OPAA enzyme was derived from Alteromonas strain JD6. It has broad substrate specificity to a wide range of OP compounds: DFP and the nerve agents, soman and sarin. Liposomes encapsulating OPAA (SL)* were made by mechanical dispersion method. Hydrolysis of DFP by (SL)* was measured by following an increase of fluoride ion concentration using a fluoride ion selective electrode. OPAA entrapped in the carrier liposomes rapidly hydrolyze DFP, with the rate of DFP hydrolysis directly proportional to the amount of (SL)* added to the solution. Liposomal carriers containing no enzyme did not hydrolyze DFP. The reaction was linear and the rate of hydrolysis was first order in the substrate. This enzyme carrier system serves as a biodegradable protective environment for the recombinant OP-metabolizing enzyme, OPAA, resulting in prolongation of enzymatic concentration in the body. These studies suggest that the protection of OP intoxication can be strikingly enhanced by adding OPAA encapsulated within (SL)* to pralidoxime and atropine.     

Aquatic Insects and Trace Metals: Bioavailability,Bioaccumulation, and Toxicity

Abstract

The uptake of metals from food and water sources by insects is thought to be additive. For a given metal, the proportions taken up from water and food will depend both on the bioavailable concentration of the metal associated with each source and the mechanism and rate by which the metal enters the insect. Attempts to correlate insect trace metal concentrations with the trophic level of insects should be made with a knowledge of the feeding relationships of the individual taxa concerned. Pathways for the uptake of essential metals, such as copper and zinc, exist at the cellular level, and other nonessential metals, such as cadmium, also appear to enter via these routes. Within cells, trace metals can be bound to proteins or stored in granules. The internal distribution of metals among body tissues is very heterogeneous, and distribution patterns tend to be both metal and taxon specific. Trace metals associated with insects can be both bound on the surface of their chitinous exoskeleton and incorporated into body tissues. The quantities of trace meals accumulated by an individual reflect the net balance between the rate of metal influx from both dissolved and particulate sources and the rate of metal efflux from the organism. The toxicity of metals has been demonstrated at all levels of biological organization: cell, tissue, individual, population, and community. Much of the literature pertaining to the toxic effects of metals on aquatic insects is based on laboratory observations and, as such, it is difficult to extrapolate the data to insects in nature. The few experimental studies in nature suggest that trace metal contaminants can affect both the distribution and the abundance of aquatic insects. Insects have a largely unexploited potential as biomonitors of metal contamination in nature. A better understanding of the physico-chemical and biological mechanisms mediating trace metal bioavailability and exchange will facilitate the development of general predictive models relating trace metal concentrations in insects to those in their environment. Such models will facilitate the use of insects as contaminant biomonitors.     

Alzheimer’s disease – current trends in basic and clinical research. Highlights from the 16th ECNP

Advances in the molecular biological knowledge of neuronal nicotinic acetylcholine receptors (nAChRs) have led to a growing interest by the pharmaceutical industry in the development of novel compounds that selectively modulate nAChR function. The ability of (-)-nicotine, an activator of nAChRs, to enhance attentional aspects of cognition in animals and humans, to exert neuroprotective and anxiolytic-like effects, and presumably to mediate the negative correlation between smoking and Alzheimer's (and Parkinson's) Disease, has focused interest on the potential therapeutic utility of modulators of nAChR function for treatment of some of the deficits associated with these progressive, neurodegenerative conditions. Numerous compounds are known which activate nAChRs and which might serve as lead compounds toward the development of such agents. The pharmacologic diversity of neuronal nAChR subtypes suggests the possibility of developing selective compounds which would have more favourable side-effect profiles than existing agents. This broader class of agents, collectively called cholinergic channel modulators (ChCMs), is anticipated to encompass compounds which would have more favourable side-effect profiles than existing agents, which generally exhibit low selectivity. This selectivity may be achieved by preferentially activating some subtypes of nAChRs (i.e., Cholinergic Channel Activators, ChCAs) or inhibiting the function of other subtypes (Cholinergic Channel Inhibitors, ChCIs). An overview of the biology of nAChRs and the rationale for the use of ChCMs for the treatment of dementia related to neurodegenerative diseases are presented, followed by a discussion of lead compounds and compounds under consideration for clinical evaluation.     

Steroidal sapogenin contents in some domestic plants

In order to find out the values of the steroid resources for the future use. the compositions and contents of steroidal sapogenins from 13 domestic plants have been investigated. As a result,Dioscorea nipponica, D. quinqueloba andSmilax china were found to have large amount of diosgenin. And pennogenin inTrillium kamtschaticum andParis verticillata, yuccagenin inAllium fistulosum, hecogenin inAgave americana and neochlorogenin inSolanum nigum were appeared to be major steroidal sapogenins.